CN103056347A - Method for controlling dendritic crystal orientation of oriented solidification structure by high-intensity magnetic field - Google Patents
Method for controlling dendritic crystal orientation of oriented solidification structure by high-intensity magnetic field Download PDFInfo
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Abstract
本发明涉及一种强磁场控制定向凝固组织枝晶取向的方法。本发明利用定向凝固过程中枝晶的择优取向和易磁化方向的差异，在定向凝固过程施加强磁场，使得枝晶受到磁化力的作用导致其易磁化轴偏向磁场方向（即定向凝固方向），从而控制合金枝晶的取向。本发明的工艺方法的要点是：利用1~14T（特斯拉）的强静磁场，采用典型Bridgman定向凝固装置，设计使定向凝固合金的固液界面处于强静磁场的中心稳恒区域，整个定向凝固过程在强静磁场下完成，采用细长的合金棒，样品固液界面的温度梯度随炉温和合金种类改变而变化。合金棒向下进行定向凝固的抽拉速率为5~100μm/s，在生长到稳定阶段后，迅速拉入冷却介质中进行淬火，最终得到枝晶生长方向发生改变的定向凝固组织。
The invention relates to a method for controlling dendrite orientation of directional solidified tissue by a strong magnetic field. The present invention utilizes the difference between the preferred orientation and easy magnetization direction of dendrites during the directional solidification process, and applies a strong magnetic field during the directional solidification process, so that the dendrites are subjected to the magnetizing force and cause their easy magnetization axes to deviate to the direction of the magnetic field (that is, the direction of directional solidification), Thereby controlling the orientation of alloy dendrites. The main points of the process method of the present invention are: utilize the strong static magnetic field of 1～14T (Tesla), adopt typical Bridgman directional solidification device, design makes the solid-liquid interface of directionally solidified alloy be in the central stable region of strong static magnetic field, the whole The directional solidification process is completed under a strong static magnetic field, using a slender alloy rod, and the temperature gradient of the solid-liquid interface of the sample changes with the furnace temperature and alloy type. The pulling rate of the alloy rod for directional solidification is 5-100 μm/s. After growing to a stable stage, it is quickly pulled into the cooling medium for quenching, and finally the directional solidification structure with the dendrite growth direction changed is obtained.
Description
技术领域 technical field
本发明涉及一种强磁场控制定向凝固组织枝晶取向的方法，属于合金组织控制研究技术领域。 The invention relates to a method for controlling dendrite orientation of a directional solidified structure by a strong magnetic field, and belongs to the technical field of alloy structure control research.
背景技术 Background technique
枝晶是材料制备成形过程中最为常见的一种组织花样，其尺寸及形态对材料的最终性能具有非常重要的影响。通常情况下，树枝晶生长的取向会尽可能与热流方向一致或相反，而且沿由晶体学确定的择优取向生长（例：Al枝晶，择优枝晶取向为<100>；Sn枝晶，择优枝晶取向为<110>）。在定向凝固的树枝晶单晶（例如涡轮叶片）中，组成这一单个晶粒的所有树枝晶都整齐地排列起来，从而改善了高温性能。 Dendrite is the most common tissue pattern in the process of material preparation, and its size and shape have a very important impact on the final performance of the material. Normally, the orientation of dendrite growth will be as consistent or opposite to the heat flow direction as possible, and grow along the preferred orientation determined by crystallography (for example: Al dendrites, the preferred dendrite orientation is <100>; Sn dendrites, the preferred dendrite orientation is <100>; Dendrite orientation is <110>). In directionally solidified dendritic single crystals, such as turbine blades, all the dendrites that make up this single grain are aligned, resulting in improved high-temperature performance.
由于定向凝固组织及单晶存在明显的各向异性现象，晶体取向对合金性能的影响也是研究热点之一。Dalal等人发现单晶SC7-14-6合金的持久性能以<111>取向时为最高。Mckay等对Mar-M247单晶在760℃蠕变性能研究表明，在晶体取向<001>及<111>方向均有较高的性能。由于高对称的晶体取向（<001>，<111>），晶体蠕变达到交叉滑移所需的晶体转动较小，经相对较小的初始蠕变状态随即进入第二蠕变阶段，因而一般具有较长的持久寿命。以上研究均表明定向凝固组织中晶体的取向直接影响材料的各项性能。目前为止，为了获得具有一定枝晶取向的材料组织，一般采用的手段是通过定向凝固籽晶法控制晶体取向，或是通过轧制获得具有一定取向织构的材料。但是籽晶法往往需要制备出具一定取向的单晶作为籽晶，需要耗费大量的人力、物力。通过轧制方法得到的材料，其织构取向度不高。 Due to the obvious anisotropy phenomenon in the directionally solidified structure and single crystal, the effect of crystal orientation on the properties of the alloy is also one of the research hotspots. Dalal et al. found that the durability of the single crystal SC7-14-6 alloy was highest in the <111> orientation. Research on the creep properties of Mar-M247 single crystal at 760 °C by Mckay et al. shows that it has high performance in the crystal orientation <001> and <111> directions. Due to the highly symmetrical crystal orientation (<001>, <111>), the crystal rotation required for crystal creep to cross-slip is small, and the relatively small initial creep state then enters the second creep stage, so generally Has a long lasting life. The above studies all show that the crystal orientation in the directionally solidified structure directly affects the properties of the material. So far, in order to obtain a material structure with a certain dendrite orientation, the general method used is to control the crystal orientation by directional solidification seed crystal method, or to obtain a material with a certain orientation texture by rolling. However, the seed crystal method often needs to prepare a single crystal with a certain orientation as the seed crystal, which requires a lot of manpower and material resources. The material obtained by the rolling method has a low degree of texture orientation.
发明内容 Contents of the invention
针对现有技术存在的不足，本发明的目的是提供一种强磁场控制定向凝固组织枝晶取向的方法。与籽晶法和轧制法对比，本方法通过在定向凝固过程中引入强磁场，强磁场将导致具有磁各向异性的晶体发生转动，导致易磁化轴方向转向磁场方向。 Aiming at the deficiencies in the prior art, the purpose of the present invention is to provide a method for controlling dendrite orientation of directional solidified tissue by a strong magnetic field. Compared with the seed crystal method and the rolling method, this method introduces a strong magnetic field during the directional solidification process, and the strong magnetic field will cause the crystal with magnetic anisotropy to rotate, causing the direction of the easy axis of magnetization to turn to the direction of the magnetic field.
为达到上述目的，本发明采用如下技术方案： To achieve the above object, the present invention adopts the following technical solutions:
一种强磁场控制定向凝固组织枝晶取向的方法，具有以下的过程和步骤： A method for controlling dendrite orientation of directional solidified tissue by a strong magnetic field has the following processes and steps:
a. 选择99.99%的高纯合金原料，配置合金成分各为Bi-0.85wt%Mn（Bi-Mn合金），Al-12wt%Ni（Al-Ni合金），Al-4.5wt%Cu（Al-Cu合金）的三种合金在真空炉中熔炼，电磁搅拌1小时，使原材料充分合金化后，用内径为3mm的石英管进行真空负压吸铸，得到枝晶生长择优取向与易磁化方向各异的Bi-Mn、Al-Ni和Al-Cu三种体系的成分均匀的合金棒试样，并将其封装在刚玉坩埚中； a. Select 99.99% high-purity alloy raw materials, and configure the alloy components as Bi-0.85wt%Mn (Bi-Mn alloy), Al-12wt%Ni (Al-Ni alloy), Al-4.5wt%Cu (Al- Cu alloy) were smelted in a vacuum furnace and stirred electromagnetically for 1 hour to fully alloy the raw materials, then vacuum negative pressure suction casting was carried out with a quartz tube with an inner diameter of 3 mm to obtain the preferred orientation of dendrite growth and the direction of easy magnetization. Alloy rod samples with uniform composition of different Bi-Mn, Al-Ni and Al-Cu systems were packaged in corundum crucibles;
b. 将传统常规定向凝固装置放入超导强静磁场发生体内，超导磁体产生的静磁场强度范围为1~14T；将刚玉坩埚放置于定向凝固装置的拉杆上，使其能在加热炉中抽拉作垂直移动；加热使合金熔化，保温0.5小时后，开启抽拉系统以设定的拉速进行定向抽拉；试样定向凝固方向与磁场方向平行，凝固界面前沿液相的温度梯度随加热炉温度变化而变化；Bi-Mn合金定向凝固过程中加热炉中心炉温为650℃，固液界面前沿的温度梯度为50K/cm；Al-Ni和Al-Cu合金的加热炉中心炉温为900℃，温度梯度分别为38K/cm和68K/cm；在抽拉过程中保证固液界面处于稳恒磁场区域； b. Put the traditional conventional directional solidification device into the superconducting strong static magnetic field generating body. The static magnetic field strength generated by the superconducting magnet ranges from 1 to 14T; place the corundum crucible on the pull rod of the directional solidification device so that it can The center pull is used to move vertically; the alloy is heated to melt, and after 0.5 hours of heat preservation, the pull system is turned on to perform directional pull at the set pulling speed; the directional solidification direction of the sample is parallel to the direction of the magnetic field, and the temperature gradient of the liquid phase at the front of the solidification interface It changes with the temperature of the heating furnace; the central furnace temperature of the heating furnace during the directional solidification of the Bi-Mn alloy is 650 ° C, and the temperature gradient at the front of the solid-liquid interface is 50 K/cm; the central furnace of the heating furnace of the Al-Ni and Al-Cu alloys The temperature is 900°C, and the temperature gradients are 38K/cm and 68K/cm respectively; during the drawing process, the solid-liquid interface is guaranteed to be in a stable magnetic field area;
c. 抽拉至稳定生长时，迅速拉入Ga-In-Sn淬火池中进行淬火，得到枝晶生长方向发生改变的定向凝固柱状晶组织。 c. When pulling to stable growth, quickly pull into the Ga-In-Sn quenching pool for quenching, and obtain the directionally solidified columnar crystal structure with the dendrite growth direction changed.
本发明方法采用传统常规的定向凝固装置，包括保护气氛输入管、水冷套管、加热炉、控温装置、合金棒试样、超导强磁体、淬火池、刚玉坩埚以及拉杆；放置有合金棒试样的刚玉坩埚放置在加热炉内；加热炉的外侧安装有水冷套管，超导强磁体置于水冷套管的外侧，且磁场方向与定向凝固方向相平行；合金定向凝固过程中固液界面置于超导强磁体的稳恒区域；加热炉连接控温装置控制其温度；在加热炉顶端有一通入惰性气体的保护气氛输入管；拉杆与刚玉坩埚连接；淬火池位于加热炉下方。 The method of the present invention adopts traditional conventional directional solidification device, including protective atmosphere input pipe, water cooling sleeve, heating furnace, temperature control device, alloy rod sample, superconducting strong magnet, quenching pool, corundum crucible and pull rod; place alloy rod The corundum crucible of the sample is placed in the heating furnace; a water-cooled sleeve is installed on the outside of the heating furnace, and a superconducting strong magnet is placed outside the water-cooled sleeve, and the direction of the magnetic field is parallel to the direction of directional solidification; during the directional solidification of the alloy, the solid-liquid The interface is placed in the stable area of the superconducting strong magnet; the heating furnace is connected to a temperature control device to control its temperature; on the top of the heating furnace there is a protective atmosphere input pipe for feeding inert gas; the tie rod is connected to the corundum crucible; the quenching pool is located under the heating furnace.
本发明的原理是基于具有各向异性的晶体，在磁场中会发生取向。假设一个具有各向异性的晶体处于磁场中，单位体积的磁矩可以表示为： The principle of the invention is based on anisotropic crystals, which are oriented in a magnetic field. Assuming an anisotropic crystal is in a magnetic field, the magnetic moment per unit volume can be expressed as:
其中，θ为c轴与磁场方向的夹角，当磁场发生变化时，放在其中的磁各向异性晶体的磁化能改变为: Among them, θ is the angle between the c-axis and the direction of the magnetic field. When the magnetic field changes, the magnetization energy of the magnetic anisotropic crystal placed therein changes as:
将式(2)和式(3)代入式(4)得 Substitute formula (2) and formula (3) into formula (4) to get
积分得: Points get:
将
这里
当
(8) (8)
当
当
与现有技术相比，本发明具有如下突出的实质性特点和显著的进步： Compared with the prior art, the present invention has the following outstanding substantive features and remarkable progress:
本方法是一种通过控制磁场强度和定向凝固速度改变定向凝固组织枝晶取向的新方法，本发明在合金定向凝固过程中施加轴向强磁场，发现对于定向凝固择优生长方向与晶体易磁化方向不同的晶体，磁场的施加导致枝晶组织取向发生改变。本方法只要在现在工业上广泛使用的高速凝固方法施加静磁场就能达到目的，操作简单且易于实现。 This method is a new method for changing the dendrite orientation of the directional solidification structure by controlling the magnetic field strength and directional solidification speed. The invention applies a strong axial magnetic field during the directional solidification of the alloy, and finds that the preferred growth direction and crystal magnetization direction are preferred for directional solidification. Different crystals, the application of a magnetic field leads to changes in the orientation of dendrites. The method can achieve the purpose as long as the static magnetic field is applied to the high-speed solidification method widely used in industry, and the operation is simple and easy to realize.
附图说明 Description of drawings
图1为本发明所利用的传统常规的强磁场下Bridgman法定向凝固装置示意图。 FIG. 1 is a schematic diagram of a conventional Bridgman method directional solidification device under a strong magnetic field used in the present invention.
图2为本发明方法的原理示意图，其中（a）、（b）和（c）分别为晶体易磁化轴方向与择优生长方向平行、有一定夹角和垂直三种情况下，施加强磁场对枝晶生长取向的作用。 Fig. 2 is a schematic diagram of the principle of the method of the present invention, wherein (a), (b) and (c) are three cases where the direction of the easy magnetization axis of the crystal is parallel to the preferred growth direction, has a certain angle and is perpendicular to the direction of the crystal. The role of dendrite growth orientation.
图3分别为Bi-0.82wt%Mn、Al-4.5wt%Cu和Al-12wt%Ni三种初生相枝晶性能各异的合金在有无强磁场作用下的定向凝固纵截面的组织。 Figure 3 shows the microstructures of the directionally solidified longitudinal sections of alloys with three primary phase dendrites, Bi-0.82wt%Mn, Al-4.5wt%Cu and Al-12wt%Ni, with and without strong magnetic field.
具体实施方式 Detailed ways
下面结合附图将本发明的具体实施例叙述于后。 Specific embodiments of the present invention will be described below in conjunction with the accompanying drawings.
实施例1Example 1
实施材料选择初生相为MnBi晶体的Bi-0.82wt%Mn合金。按照合金比例称量纯Bi和纯Mn金属，在真空炉中进行熔炼。电磁搅拌1小时后，用内径为3mm的石英管进行负压吸铸，得到成分均匀的合金棒，并将其封装在刚玉管中。刚玉管装在拉杆上，拉杆连接定向凝固伺服抽拉系统。设计使试样的固液界面处于强磁体稳恒磁场区域，定向凝固装置为典型的Bridgman装置。伺服抽拉系统设置的拉速为5μm/s、温度梯度为50K/cm、在磁场强度为10T下进行定向凝固。定向凝固的试样在抽拉8cm后，达到稳定生长区域，这时以一较大拉速迅速拉入Ga-In-Sn淬火池中进行淬火。将所得的定向凝固试样在固液界面下方对称切开，得到观察组织的纵截面样品，镶嵌样品后，经过研磨、抛光后腐蚀观察组织。 The implementation material selects Bi-0.82wt%Mn alloy whose primary phase is MnBi crystal. The pure Bi and pure Mn metals are weighed according to the alloy ratio, and melted in a vacuum furnace. After electromagnetic stirring for 1 hour, a quartz tube with an inner diameter of 3 mm was used for negative pressure suction casting to obtain an alloy rod with uniform composition, which was packaged in a corundum tube. The corundum tube is installed on the pull rod, and the pull rod is connected to the directional solidification servo pulling system. The design makes the solid-liquid interface of the sample in the stable magnetic field region of the strong magnet, and the directional solidification device is a typical Bridgman device. The servo pulling system was set with a pulling speed of 5 μm/s, a temperature gradient of 50K/cm, and a magnetic field strength of 10T for directional solidification. The directionally solidified sample reaches the stable growth region after being pulled for 8 cm, and then is quickly pulled into the Ga-In-Sn quenching pool at a relatively high pulling speed for quenching. The obtained directional solidification sample is symmetrically cut under the solid-liquid interface to obtain a longitudinal section sample of the observed tissue, and after the sample is mounted, the observed tissue is corroded after grinding and polishing.
实施例2Example 2
本实施例的过程和步骤与上述实施例1基本相同。特别之处在于：采用的合金为Al-4.5wt%Cu，初生相为α-Al。定向凝固抽拉速度为50μm/s，加热炉中心区域温度为900℃，温度梯度为38K/cm。
The process and steps of this embodiment are basically the same as those of
实施例3Example 3
本实施例的过程和步骤与上述实施例1基本相同。特别之处在于：采用的合金为Al-12wt%Ni，初生相为Al3Ni。定向凝固抽拉速度为100μm/s，加热炉中心区域温度为900℃，温度梯度为68K/cm，磁场强度为12T。
The process and steps of this embodiment are basically the same as those of
三个实施例分别选了择优生长方向与易磁化方向相同、存在一定夹角和垂直的三种晶体作为研究对象。图2显示的分别是上述三种情况下，磁场的作用导致枝晶的生长发生改变的示意图，实线箭头表示晶体的择优生长方向，虚线箭头表示晶体的易磁化轴方向。对于择优生长方向与易磁化方向相同的MnBi初生相，晶体在磁场下受到的电磁力将诱导MnBi沿磁场方向生长；对于Al-4.5wt%Cu合金，其初生相枝晶为α-Al，其择优生长方向为<100>，其易磁化方向为<111>，在磁场的作用下，枝晶将发生偏转，易磁化方向<111>沿着定向凝固方向排列。对于Al-12wt%Ni合金，初生相Al3Ni的择优生长方向与易磁化方向垂直，这种合金的枝晶在磁场的作用下，其生长方向可以垂直于磁场方向。图3为上述三个实施例的纵截面定向凝固组织照片。 In the three examples, three kinds of crystals whose preferred growth direction is the same as the easy magnetization direction, have a certain included angle and are perpendicular to each other are selected as research objects. Figure 2 shows the schematic diagrams of the changes in the growth of dendrites caused by the action of the magnetic field in the above three cases, the solid arrows indicate the preferred growth direction of the crystal, and the dotted arrows indicate the direction of the easy magnetization axis of the crystal. For the MnBi primary phase whose preferred growth direction is the same as the easy magnetization direction, the electromagnetic force on the crystal under the magnetic field will induce MnBi to grow along the magnetic field direction; for the Al-4.5wt%Cu alloy, the primary phase dendrite is α-Al, and its The preferred growth direction is <100>, and its easy magnetization direction is <111>. Under the action of the magnetic field, the dendrite will deflect, and the easy magnetization direction <111> is arranged along the direction of directional solidification. For the Al-12wt%Ni alloy, the preferred growth direction of the primary phase Al 3 Ni is perpendicular to the direction of easy magnetization, and the growth direction of the dendrites of this alloy can be perpendicular to the direction of the magnetic field under the action of the magnetic field. Fig. 3 is a photo of the longitudinal section directional solidified tissue of the above three embodiments.
在磁场下的定向凝固过程中，具有各向异性的晶体将会沿其择优取向方向生长，但同时晶体的易磁化轴将转向磁场方向。当易磁化轴方向与择优生长方向相同时，轴向磁场将提高定向凝固方向的生长。实施例1中，MnBi晶体的<001>方向不仅是易磁化轴方向也是择优生长方向，因此定向凝固过程中磁场的施加会促进枝晶沿定向凝固方向的生长。实施例2中，Al-4.5wt%Cu合金中，Al晶体的易磁化轴方向和择优生长方向分别是<111>和<100>方向，因此在10T磁场作用下，Al晶体<111>方向转向定向凝固方向。在特殊情况下，如实施例3，Al3Ni晶体易磁化轴与择优取向方向垂直，磁场的作用导致择优生长方向垂直于定向凝固方向，形成了层状结构。 During directional solidification under a magnetic field, an anisotropic crystal will grow along its preferred orientation, but at the same time the crystal's easy axis of magnetization will turn to the direction of the magnetic field. When the axis of easy magnetization is in the same direction as the preferred growth direction, the axial magnetic field will enhance the growth in the direction of directional solidification. In Example 1, the <001> direction of the MnBi crystal is not only the direction of the easy magnetization axis but also the preferred growth direction, so the application of a magnetic field during the directional solidification process will promote the growth of dendrites along the directional solidification direction. In Example 2, in the Al-4.5wt%Cu alloy, the direction of the easy magnetization axis and the preferred growth direction of the Al crystal are the <111> and <100> directions respectively, so under the action of a 10T magnetic field, the direction of the Al crystal <111> turns to Directional solidification direction. In a special case, as in Example 3, the easy magnetization axis of Al 3 Ni crystals is perpendicular to the preferred orientation direction, and the action of the magnetic field causes the preferred growth direction to be perpendicular to the directional solidification direction, forming a layered structure.
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